CN103556134A - Pre-treatment method of non-electrolytic nickel plating - Google Patents
Pre-treatment method of non-electrolytic nickel plating Download PDFInfo
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Abstract
The invention provides a pre-treatment method of non-electrolytic nickel plating. The pre-treatment method comprises the following steps: cleaning and coarsening a substrate with a copper surface by a microetching liquid to obtain the substrate with the coarsened copper surface; then, enabling the substrate with the coarsened copper surface to be in contact with a pre-treatment combined liquid to obtain the treated substrate with the copper surface, wherein the pre-treatment combined liquid comprises an acid, a reducer and water; and then, activating the treated substrate with the copper surface by an ionic palladium activating liquid. Compared with the prior art, the pre-treatment combined liquid containing the acid and the reducer is in contact with the copper surface of the substrate, the pre-treatment combined liquid can reduce the copper ion containing liquor falling into gaps between the copper surface and a high molecular non-plating area in advance to cuprous oxide salt which is easy to be dissolved in weak acids, and the cuprous oxide salt can be dipped, washed and cleaned by the weak acid which is not activated by palladium, so that hydrolyzed hydroxide of suspended palladium cores or palladium cannot be formed when the ionic palladium activating liquid is used to activate, thereby avoiding the problem of residual nickel plating.
Description
Technical field
The invention belongs to chemical nickel and gold or chemical nickel porpezite technical field of surface, relate in particular to the pretreatment process of process for electroless nickel plating.
Background technology
Desired being not only of high-density electronic packaging and circuit board technology made less hole, more fine and closely woven circuit, more smooth weld pad, and the final surface treatment of circuit card must provide can weld, can routing, and have and can maintain the functions such as low contact resistance.
Now, the selectable final surface treatment of copper face that anti-solder ink exposes has chemical nickel and gold technique and chemical nickel porpezite technique.These two kinds of process of surface treatment all have concurrently can weld, can contact conducting, can routing with can assist the multi-functionals such as heat radiation, can meet the processing procedure of multiple demand.And, the treating processes of these two kinds of techniques is all the chemical Ni-P alloy of plating one deck 3～5 μ m in the copper wire of printed circuit board (PCB) or copper pad, as blocking metal ion transport between displacement gold and substrate copper or the barrier layer of diffusion, the while also can be avoided oxidation affects solderability and the wettability of copper face.
Because cannot directly driving the deposition reaction of chemical nickel, copper surface carries out process for electroless nickel plating, therefore need first with palladium copper surface active, utilize copper to be greater than the ionization trend of palladium, the electronics discharging after copper dissolution makes palladium ion be reduced into metallic state, in copper surface replacement, form thin palladium crystal seed layer, the catalyst that the palladium of usining reacts as chemical nickel, impels Hypophosphite oxidation.
Between palladium activation and chemical nickel, must fully clean printed circuit board (PCB), to remove, may attach in the suspension palladium core of non-plating face (as anti-solder ink or exposed board substrate or the imageable dry film of light) or the lioh hydrolysis compound of palladium.These metallic palladium that attach on non-plating face may cause unnecessary nickel deposition, when slight, produce the nickel of being stained with of shape fragmentarily, when serious, will cause copper surface to be filled out or plating around, more serious in the bridge formation short circuit causing between circuit or between weld pad, especially on the small weld pad of high density distribution and fine rule road, this bridge formation short circuit may make it test by 5 ℃/85 ℃ relative humidity or the high reliability that accelerates humiture.
In order to strengthen the cleaning performance between palladium activation and chemical nickel, to use sometimes 1～2% sulfuric acid as rear pickling, with those faint metallic palladium that are attached in Fei Du district of assist in dissolving, just enter chemical nickel step through twice water-washing step more afterwards.Yet rear pickling must be diligent in changing, otherwise not only cannot reach the effect of cleaning, can suspend because of the palladium core of accumulation on the contrary, may cause the palladium absorption in Fei Du district.
The solution of the unnecessary nickel plating in Fei Du district, mainly contains following methods now:
The palladium activated solution of the research such as Watanable, utilize ammonium chloride as the complex compound of palladium, and add anion surfactant-sodium lauryl sulphate as wetting agent, good palladium-the chloro-complex of complexing can avoid producing in palladium activated solution the oxyhydroxide of palladium, be adsorbed on simultaneously copper surface around the anion surfactant of insulating regions also can repel (the K.Watanabe that adheres to of palladium-chloro-complex, T.Nishiwaki, H.Honma, the 55th annual meeting of International Society of Electrochemistry-, Thessaloniki, in September, 2004 19-24).Yet the complex compound that palladium-chloro-complex and part water molecules replace can form anionic title complex, or water molecules all replaces and becomes hydrated cation title complex, cause diffusion to weaken, Fei Du district forms large-scale gathering together, and causes plating, and these are gathered together and are also difficult to water and remove.
The patent No. be JP241853 Japanese Patent Publication a kind of palladium activation solution, comprise chlorion, palladium ion and contain displacement promotor, displacement promotor is hypophosphite, phosphite, hydrazine hydrate, azanol, borine or formaldehyde, and the acidity of activation solution is defined as more than 0.1.But displacement promotor has reductibility, easily causes palladium ion and is reduced into palladium atom and is suspended in activation solution, unsettled palladium atom more easily causes the problem of the unnecessary nickel plating in Fei Du district.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of pretreatment process of process for electroless nickel plating, and this pretreatment process can suppress to occur the problem of unnecessary nickel plating.
The pretreatment process that the invention provides a kind of process for electroless nickel plating, comprising:
A) with micro-etching solution, the substrate of copper containing surfaces is cleaned and alligatoring, obtained the substrate after copper surface coarsening;
B) substrate after described copper surface coarsening is contacted to the substrate of the copper containing surfaces after being processed with pre-treatment combination liquid; Described pre-treatment combination liquid comprises acid, reductive agent and water;
C) after the substrate with the copper containing surfaces after processing described in weak acid preimpregnation, then activate with ionic palladium activation solution.
Preferably, described pre-treatment combination liquid also comprises wetting agent.
Preferably, described wetting agent is selected from one or more in nonionogenic tenside, cats product and amphoterics.
Preferably, the concentration of described wetting agent is 0.1～10g/L.
Preferably, the acid of described pre-treatment combination liquid is selected from one or more in sulfuric acid, hydrochloric acid, toluenesulphonic acids and phenmethyl sulfonic acid.
Preferably, the sour concentration of described pre-treatment combination liquid is 10～150g/L.
Preferably, the reductive agent of described pre-treatment combination liquid is selected from one or more in glucose, hydrazine hydrate and azanol.
Preferably, the concentration of the reductive agent of described pre-treatment combination liquid is 1～50g/L.
Preferably, the temperature contacting in described step B is 20 ℃～50 ℃, and the time of contact is 60～500s.
Preferably, described step B also comprises: after the substrate of the copper containing surfaces after being processed, wash.
The invention provides a kind of pretreatment process of process for electroless nickel plating, with micro-etching solution, the substrate of copper containing surfaces is cleaned and alligatoring, obtain the substrate after copper surface coarsening; Then the substrate after described copper surface coarsening is contacted to the substrate of the copper containing surfaces after being processed with pre-treatment combination liquid; Described pre-treatment combination liquid comprises acid, reductive agent and water; With ionic palladium activation solution, activate again the substrate of the copper containing surfaces after described processing.Compared with prior art, the present invention contacts the copper surface of substrate with the pre-treatment combination liquid of reductive agent with comprising acid, pre-treatment combination liquid can will be subside the Red copper oxide salt that becomes to be soluble in weak acid in the copper ions solution pre-reduction in gap between copper surface and polymer Fei Du district, weak acid before its available palladium activation embathes and cleans up, and then make the activation of ionic palladium activation solution time cannot form the lioh hydrolysis compound of suspension palladium core or palladium, thereby can avoid occurring the problem of unnecessary nickel plating.
Embodiment
The pretreatment process that the invention provides a kind of process for electroless nickel plating, comprising:
A) with micro-etching solution, the substrate of copper containing surfaces is cleaned and alligatoring, obtained the substrate after copper surface coarsening;
B) substrate after described copper surface coarsening is contacted to the substrate of the copper containing surfaces after being processed with pre-treatment combination liquid; Described pre-treatment combination liquid comprises acid, reductive agent and water;
C) after the substrate with the copper containing surfaces after processing described in weak acid preimpregnation, then activate with ionic palladium activation solution.
The present invention does not have special restriction to the source of all raw materials, for commercially available.
Wherein, described micro-etching solution is micro-etching solution well known to those skilled in the art, can be sulfuric acid-Sodium Persulfate system and also can be sulfuric acid-hydrogen peroxide system, there is no special restriction.The substrate of described copper containing surfaces is substrate well known to those skilled in the art, can be printed-wiring board (PWB), there is no special restriction.Micro-etching solution to the substrate of copper containing surfaces clean with alligatoring after, containing the high micro-etching solution of bivalent cupric ion, easily form copper oxide or copper oxyhydroxide, these are trapped in space or the interval between copper surface and polymer Fei Du district containing the high solution of bivalent cupric ion, being difficult to use thoroughly cleans up, follow-up when by this substrate immersion plating during in ionic palladium activation solution, in the situation that palladium ion free state is high, can become nano copper particle by the above-mentioned cupric salt fast restore of catalysis, and make palladium ion and nano copper particle displacement separate out palladium atom thereupon, with coated Nanometer Copper (core)/palladium (shell) bimetal granule that forms in nano copper particle surface, subsequent chemistry nickel can form chemical nickel deposition at this because of the catalysis of palladium, form unnecessary plating.
Wherein said copper surface is for being positioned at suprabasil copper wire or copper pad; Described polymer Fei Du district is positioned at substrate to comprise anti-solder ink, exposed base material or the imageable dry film of light.
Obtain after the substrate after copper surface coarsening, it is contacted to the substrate of the copper containing surfaces after being processed with pre-treatment combination liquid.Wherein, described pre-treatment combination liquid comprises acid, reductive agent and water; Described acid can be mineral acid and also can be organic acid, there is no special restriction, is preferably one or more in mineral acid or organic acid, more preferably one or more in sulfuric acid, hydrochloric acid, toluenesulphonic acids and phenmethyl sulfonic acid; The concentration of described acid in pre-treatment combination liquid is preferably 10～150g/L, more preferably 20～50g/L; Described reductive agent is the compound with reductibility well known to those skilled in the art, there is no special restriction, is preferably one or more in glucose, hydrazine hydrate and azanol in the present invention; The concentration of described reductive agent in pre-treatment combination liquid is preferably 1～50g/L, more preferably 10～30g/L.
The pre-treatment combination liquid that comprises acid and reductive agent can by subside in copper surperficial with polymer Fei Du district between the copper ions solution pre-reduction in gap become to be soluble in the Red copper oxide salt of weak acid, weak acid before its available palladium activation embathes and cleans up, and then make the activation of ionic palladium activation solution time cannot form the lioh hydrolysis compound of suspension palladium core or palladium, thereby can avoid occurring the problem of unnecessary nickel plating.
According to the present invention, described pre-treatment combination liquid preferably also comprises wetting agent, can reduce the infiltration surface tension of the substrate after copper surface coarsening, in the present invention, be preferably one or more in nonionogenic tenside, cats product and amphoterics; The concentration of described wetting agent in pre-treatment combination liquid is preferably 0.1～10g/L, 0.5～8g/L more preferably, then be preferably 1～5g/L.
Substrate after described copper surface coarsening contacts with pre-treatment combination liquid, and wherein, the temperature of described contact is preferably 20 ℃～50 ℃, is preferably 30 ℃～40 ℃; The time of described contact is preferably 60～500s, more preferably 180～300s.
After the substrate of the copper containing surfaces after the present invention is preferably processed, wash.The water quality of described washing is selected from deionized water, ion exchange pure water or reverse osmosis pure water.Washing clearly surface removes remaining pre-treatment combination liquid, the suprabasil pre-treatment combination liquid of thoroughly removing remaining copper containing surfaces after processing is necessary, otherwise the reductive agent in pre-treatment combination liquid is brought in ionic palladium activation solution, easily cause that the luxus consumption of palladium activation solution and palladium separate out phenomenon.
Substrate with the copper containing surfaces after processing described in weak acid preimpregnation, described weak acid is acid identical in ionic palladium activation solution, after weak acid preimpregnation, without washing, directly enter in ionic palladium activation solution, can maintain the acidity in palladium activation solution, also can make it before entering palladium activation solution, keep the fresh state (oxide-free) on copper surface simultaneously.
With ionic palladium activation solution, activate, wherein said ionic palladium activation solution is ionic palladium activation solution well known to those skilled in the art, there is no special restriction.The activation solution of ionic palladium described in the present invention preferably comprises inorganic or organic acid, palladium salt and tensio-active agent; Described inorganic or organic acid is preferably one or more in hydrochloric acid, sulfuric acid, methylsulphonic acid and phenmethyl sulfonic acid; Inorganic or organic acid concentration is preferably 10～200g/L, more preferably 20～100g/L; Described palladium salt is preferably one or more in Palladous chloride, palladous sulfate and palladium; Wherein the concentration of palladium ion in ionic palladium activation solution is preferably 10～100mg/L, more preferably 20～50mg/L; Described tensio-active agent is tensio-active agent well known to those skilled in the art, there is no special restriction.
The temperature of intermediate ion palladium activation solution activation of the present invention is preferably 20 ℃～35 ℃, more preferably 25 ℃～30 ℃; The time of activation is preferably 30～500s, more preferably 120～300s.
After the activation of ionic palladium activation solution, can carry out those skilled in the art and know process for electroless nickel plating, on the copper surface of palladium ion activation solution activation, implement chemical nickel.
In order to further illustrate the present invention, below in conjunction with embodiment, the pretreatment process of process for electroless nickel plating provided by the invention is described in detail.
In following examples, reagent used is commercially available.
Embodiment 1
The printed wiring base board with 150 μ m copper wire and anti-solder ink is processed through following successively: in the solution containing chemical pure sulfuric acid 15ml/L and citric acid 10g/L, 40 ℃ of immersion 5min carry out pickling degreasing, by deionized water normal temperature washed twice, each washing 1min, after two washings, substrate 30 ℃ of immersion 1.5min in the micro-etching solution containing chemical pure sulfuric acid 25ml/L and Sodium Persulfate 80g/L are carried out to microetch processing, use again deionized water normal temperature washed twice, each washing 1min, then under 40 ℃ of conditions with containing chemical pure level sulfuric acid 90g/L, the pre-treatment combination immersion bubble 4min of oxammonium sulfate 25g/L and water, deionized water normal temperature washed twice, each washing 1min, with under 7.5ml/L chemical pure sulphuric acid soln normal temperature, substrate being carried out to pre-pickling 1min, with the about 15mg/L of chloride containing palladium 25mg/L(palladium ion) with 25 ℃ of activation 3min of the ionic palladium activation solution of chemical pure sulfuric acid 15ml/L, use again deionized water normal temperature washed twice, each washing 1min, finally use chemical Ni-P alloy electroplating bath (Shenzhen Hua Xun Applied Materials Inc, chemical nickel EN-52 series) in 84 ℃ of immersion plating 20min, deposit the nickel deposited phosphorus alloy (phosphorus content approximately 8%) of approximately 3.5 μ m left and right, obtain the substrate of nickel deposited phosphorus alloy.
Utilize opticmicroscope to analyze the substrate of the nickel deposited phosphorus alloy obtaining in embodiment 1, find the phenomenon that copper wire does not have unnecessary nickel plating to ooze out completely around.
Embodiment 2
The printed wiring base board with 150 μ m copper wire and anti-solder ink is processed through following successively: in the solution containing chemical pure sulfuric acid 15ml/L and citric acid 10g/L, 40 ℃ of immersion 5min carry out pickling degreasing, by deionized water normal temperature washed twice, each washing 1min, after two washings, substrate 30 ℃ of immersion 1.5min in the micro-etching solution containing chemical pure sulfuric acid 25ml/L and Sodium Persulfate 80g/L are carried out to microetch processing, use again deionized water normal temperature washed twice, each washing 1min, then under 30 ℃ of conditions with containing chemical pure level sulfuric acid 100g/L, the pre-treatment combination immersion bubble 4min of oxammonium sulfate 15g/L and water, deionized water normal temperature washed twice, each washing 1min, with under 7.5ml/L chemical pure sulphuric acid soln normal temperature, substrate being carried out to pre-pickling 1min, with the about 15mg/L of chloride containing palladium 25mg/L(palladium ion) with 25 ℃ of activation 3min of the ionic palladium activation solution of chemical pure sulfuric acid 15ml/L, use again deionized water normal temperature washed twice, each washing 1min, finally use chemical Ni-P alloy electroplating bath (Shenzhen Hua Xun Applied Materials Inc, chemical nickel EN-52 series) in 84 ℃ of immersion plating 20min, deposit the nickel deposited phosphorus alloy (phosphorus content approximately 8%) of approximately 3.5 μ m left and right, obtain the substrate of nickel deposited phosphorus alloy.
Utilize opticmicroscope to analyze the substrate of the nickel deposited phosphorus alloy obtaining in embodiment 2, find the phenomenon that copper wire does not have unnecessary nickel plating to ooze out completely around.
Embodiment 3
The printed wiring base board with 150 μ m copper wire and anti-solder ink is processed through following successively: in the solution containing chemical pure sulfuric acid 15ml/L and citric acid 10g/L, 40 ℃ of immersion 5min carry out pickling degreasing, by deionized water normal temperature washed twice, each washing 1min, after two washings, substrate 30 ℃ of immersion 1.5min in the micro-etching solution containing chemical pure sulfuric acid 25ml/L and Sodium Persulfate 80g/L are carried out to microetch processing, use again deionized water normal temperature washed twice, each washing 1min, then under 40 ℃ of conditions with containing chemical pure level sulfuric acid 100g/L, the pre-treatment combination immersion bubble 4min of glucose 10g/L and water, deionized water normal temperature washed twice, each washing 1min, with under 7.5ml/L chemical pure sulphuric acid soln normal temperature, substrate being carried out to pre-pickling 1min, with the about 15mg/L of chloride containing palladium 25mg/L(palladium ion) with 25 ℃ of activation 3min of the ionic palladium activation solution of chemical pure sulfuric acid 15ml/L, use again deionized water normal temperature washed twice, each washing 1min, finally use chemical Ni-P alloy electroplating bath (Shenzhen Hua Xun Applied Materials Inc, chemical nickel EN-52 series) in 84 ℃ of immersion plating 20min, deposit the nickel deposited phosphorus alloy (phosphorus content approximately 8%) of approximately 3.5 μ m left and right, obtain the substrate of nickel deposited phosphorus alloy.
Utilize opticmicroscope to analyze the substrate of the nickel deposited phosphorus alloy obtaining in embodiment 3, find that copper wire has slight unnecessary nickel plating to ooze out phenomenon around, and have desultory discontinuous coating, this may be due to Reduction of Glucose power in this pre-treatment combination liquid slightly weak due to.
Embodiment 4
The printed wiring base board with 150 μ m copper wire and anti-solder ink is processed through following successively: in the solution containing chemical pure sulfuric acid 15ml/L and citric acid 10g/L, 40 ℃ of immersion 5min carry out pickling degreasing, by deionized water normal temperature washed twice, each washing 1min, after two washings, substrate 30 ℃ of immersion 1.5min in the micro-etching solution containing chemical pure sulfuric acid 25ml/L and Sodium Persulfate 80g/L are carried out to microetch processing, use again deionized water normal temperature washed twice, each washing 1min, then under 40 ℃ of conditions with containing methylsulphonic acid 50g/L, the pre-treatment combination immersion bubble 4min of hydrazine hydrate 20g/L and water, deionized water normal temperature washed twice, each washing 1min, with under 7.5ml/L chemical pure sulphuric acid soln normal temperature, substrate being carried out to pre-pickling 1min, with the about 15mg/L of chloride containing palladium 25mg/L(palladium ion) with 25 ℃ of activation 3min of the ionic palladium activation solution of chemical pure sulfuric acid 15ml/L, use again deionized water normal temperature washed twice, each washing 1min, finally use chemical Ni-P alloy electroplating bath (Shenzhen Hua Xun Applied Materials Inc, chemical nickel EN-52 series) in 84 ℃ of immersion plating 20min, deposit the nickel deposited phosphorus alloy (phosphorus content approximately 8%) of approximately 3.5 μ m left and right, obtain the substrate of nickel deposited phosphorus alloy.
Utilize opticmicroscope to analyze the substrate of the nickel deposited phosphorus alloy obtaining in embodiment 4, find the phenomenon that copper wire does not have unnecessary nickel plating to ooze out completely around.
Comparative example 1
The printed wiring base board with 150 μ m copper wire and anti-solder ink is processed through following successively: in the solution containing chemical pure sulfuric acid 15ml/L and citric acid 10g/L, 40 ℃ of immersion 5min carry out pickling degreasing, by deionized water normal temperature washed twice, each washing 1min, after two washings, substrate 30 ℃ of immersion 1.5min in the micro-etching solution containing chemical pure sulfuric acid 25ml/L and Sodium Persulfate 80g/L are carried out to microetch processing, use again deionized water normal temperature washed twice, each washing 1min, then with under 7.5ml/L chemical pure sulphuric acid soln normal temperature, substrate being carried out to pre-pickling 1min, with the about 15mg/L of chloride containing palladium 25mg/L(palladium ion) with 25 ℃ of activation 3min of the ionic palladium activation solution of chemical pure sulfuric acid 15ml/L, use again deionized water normal temperature washed twice, each washing 1min, finally use chemical Ni-P alloy electroplating bath (Shenzhen Hua Xun Applied Materials Inc, chemical nickel EN-52 series) in 84 ℃ of immersion plating 20min, deposit the nickel deposited phosphorus alloy (phosphorus content approximately 8%) of approximately 3.75 μ m left and right, obtain the substrate of nickel deposited phosphorus alloy.
Utilize opticmicroscope to analyze the substrate of the nickel deposited phosphorus alloy obtaining in comparative example 1, find that copper wire the unnecessary nickel plating that similar burr fill out has occurred and oozed out phenomenon around, ooze out width approximately 30～40 μ m.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a pretreatment process for process for electroless nickel plating, is characterized in that, comprising:
A) with micro-etching solution, the substrate of copper containing surfaces is cleaned and alligatoring, obtained the substrate after copper surface coarsening;
B) substrate after described copper surface coarsening is contacted to the substrate of the copper containing surfaces after being processed with pre-treatment combination liquid; Described pre-treatment combination liquid comprises acid, reductive agent and water;
C) after the substrate with the copper containing surfaces after processing described in weak acid preimpregnation, then activate with ionic palladium activation solution.
2. pretreatment process according to claim 1, is characterized in that, described pre-treatment combination liquid also comprises wetting agent.
3. pretreatment process according to claim 2, is characterized in that, described wetting agent is selected from one or more in nonionogenic tenside, cats product and amphoterics.
4. pretreatment process according to claim 2, is characterized in that, the concentration of described wetting agent is 0.1～10g/L.
5. pretreatment process according to claim 1, is characterized in that, the acid of described pre-treatment combination liquid is selected from one or more in sulfuric acid, hydrochloric acid, toluenesulphonic acids and phenmethyl sulfonic acid.
6. pretreatment process according to claim 1, is characterized in that, the sour concentration of described pre-treatment combination liquid is 10～150g/L.
7. pretreatment process according to claim 1, is characterized in that, the reductive agent of described pre-treatment combination liquid is selected from one or more in glucose, hydrazine hydrate and azanol.
8. pretreatment process according to claim 1, is characterized in that, the concentration of the reductive agent of described pre-treatment combination liquid is 1～50g/L.
9. pretreatment process according to claim 1, is characterized in that, the temperature contacting in described step B is 20 ℃～50 ℃, and the time of contact is 60～500s.
10. pretreatment process according to claim 1, is characterized in that, described step B also comprises: after the substrate of the copper containing surfaces after being processed, wash.
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| CN104593751A (en) * | 2014-12-27 | 2015-05-06 | 广东致卓精密金属科技有限公司 | Ultralow-concentration ion palladium activation solution and process for chemical nickel-plating on copper surface |
| CN104878422A (en) * | 2014-02-28 | 2015-09-02 | 比亚迪股份有限公司 | Palladium activating solution, preparation method thereof, and plastic activating method |
| CN106987830A (en) * | 2017-04-11 | 2017-07-28 | 深圳市创智成功科技有限公司 | Aluminium base printed wiring board chemistry NiPdAu technique |
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